U.S. patent number 3,746,012 [Application Number 05/218,488] was granted by the patent office on 1973-07-17 for method of making expanded reconstituted tobacco.
Invention is credited to Edward John Deszyck.
United States Patent |
3,746,012 |
Deszyck |
July 17, 1973 |
**Please see images for:
( Certificate of Correction ) ** |
METHOD OF MAKING EXPANDED RECONSTITUTED TOBACCO
Abstract
An expanded reconstituted tobacco product is produced by forming
a slurry of tobacco plant parts and a binder of tobacco derived
pectins in an aqueous medium into which a relatively small amount
of low boiling alkanes or volatile aliphatic hydrocarbons are
dispersed. An emulsifying agent may be added to obtain a better
dispersion. The mixture is cast into sheet or web form and is then
rapidly heated to a temperature sufficient to volatilize out
substantially all of the hydrocarbons and water thereby producing a
porous spongy tobacco product of increased thickness and lower
density than an untreated reconstituted tobacco.
Inventors: |
Deszyck; Edward John (Richmond,
VA) |
Family
ID: |
22815325 |
Appl.
No.: |
05/218,488 |
Filed: |
January 17, 1972 |
Current U.S.
Class: |
131/370; 131/356;
131/353 |
Current CPC
Class: |
A24B
3/182 (20130101); A24B 15/12 (20130101) |
Current International
Class: |
A24B
3/18 (20060101); A24B 15/00 (20060101); A24B
3/00 (20060101); A24B 15/12 (20060101); A24b
003/18 () |
Field of
Search: |
;131/15,17,140-144 |
References Cited
[Referenced By]
U.S. Patent Documents
|
|
|
3364935 |
January 1968 |
Moshy et al. |
3528434 |
September 1970 |
Halter et al. |
|
Foreign Patent Documents
Primary Examiner: Rein; Melvin D.
Claims
The invention that is claimed is:
1. The method of making a reconstituted and expanded tobacco
product comprising the steps of:
a. Forming a slurry of tobacco plant particles and a binder of
tobacco derived pectins,
b. Intimately dispersing an aliphatic hydrocarbon of five to eight
carbon atoms or mixture of such hydrocarbons in an amount of about
0.007 to about 7.0 parts per 100 parts of tobacco by weight into
the tobacco slurry,
c. forming the slurry into web or sheet form,
d. Heating said tobacco slurry while in said web or sheet to a
temperature of between 150.degree. and 240.degree.F and for a time
sufficient to vaporize off water and all of said hydrocarbons and
then,
e. drying the web or sheet, said heating and drying steps effecting
a bonding of the tobacco particles and the formation of cavities or
expanded areas in and on the dried product.
2. The process of claim 1 in which the hydrocarbon is selected from
the group consisting of heptane and petroleum ether.
3. The process of claim 1, wherein at step (c) a flavoring
emulsifier is added in an amount between about 1 and 5 parts per
100 parts of tobacco fines by weight.
4. The process of claim 3, in which the emulsifier is tobacco
resins.
5. The process of claim 3, in which the emulsifier is licorice or a
salt of glycyrrhizin.
6. The process of claim 1, wherein at step (c) a non-flavoring
emulsifier is added in an amount between about 0.0002 and 0.2 parts
per 100 parts of tobacco fines by weight.
7. The process of claim 6, in which the non-flavoring emulsifier is
stearic acid or an alkaline salt thereof.
8. The process of claim 6, in which the non-flavoring emulsifier is
lauryl ether sulfate or an alkaline salt thereof.
Description
BACKGROUND OF THE INVENTION
Conventional methods of making reconstituted tobacco products
involve the casting, spraying, roll-coating or the like of a slurry
of finely-divided tobacco to form a tobacco sheet which is dried
and then processed by methods normally used in preparing filler
from reconstituted tobacco or regular tobacco leaf filler. However,
the reconstituted tobacco sheet during the drying process becomes
fairly dense and moreover quite flat in comparison to the typical
irregular shapes of natural leaf. When such a sheet is shredded to
form filler for smoking articles, the shreds are essentially flat
and these tend to pack down and result in a dense filler. Thus the
reconstituted sheet is said to have low filling power in that it
does not possess the bulk to produce a satisfactory cigarette rod.
The filling power is the ability of filler to produce a light but
firm rod, and if this can be obtained with a low density product,
filling power is increased. It should be pointed out that a dense
filler is not only uneconomical, but it will deliver more total
particulate matter (TPM) to the user.
Recognizing the problems of the usual reconstituted tobacco sheet,
it was later suggested that such a sheet be prepared with a foamed
structure to give it bulk and thus greater filling power. Various
patents of Moshy et al., notably U.S. Pat. Nos. 3,364,935;
3,404,690; 3,404,691; and 3,410,279 describe processes in which a
hydrophilic adhesive gum, capable of acting as a foaming agent, is
added to a tobacco slurry. As described in U.S. Pat. No. 3,364,935,
a mixture of tobacco and such hydrophilic adhesive gum foaming
agent together with a foam stabilizer is thoroughly beaten into an
aerated foamed mass. The foam stabilizer, of the class of
surfactants and detergents, is apparently needed to prevent
collapse of the foam with loss of air. The stabilized foamed
tobacco mixture is then dried to obtain a shaped product of desired
bulk and porosity. Should the foaming agents lack the necessary
foaming effect, the patent also suggests the use of a blowing agent
such as sodium bicarbonate to aid in producing the proper degree of
foaming.
The difficulty with such processes is that they require the
formulation of a stable foamed slurry which is generally difficult
to keep intact before the expansion step without a foam stabilizer.
Additionally, the presence of gum adhesive foaming agents and
foaming stabilizers in the final product could easily cause the
foamed tobacco sheet to possess foreign flavor notes of
questionable value due to the retention of such gums as well as the
foam stabilizers remaining in the final product. Residual alkali
material left by the "blowing" agent could also cause undesirable
effects.
A patent to Fredrickson, U.S. Pat. No. 3,524,451 describes a method
of increasing filling capacity of tobacco or tobacco parts by
soaking such material with an inert volatilizable organic foaming
agent such as hydrocarbons or halogenated hydrocarbons to fully
impregnate the tobacco. The amounts suggested by weight ratio of
liquid to tobacco may be between 1-to-3 and 3-to-1. The impregnated
tobacco with foaming agent is then contacted with a stream of hot
gases at temperatures well above the boiling point of the organic
liquid to as high as 400.degree.F. Such a procedure presumably
requires a material that stays intact when the hot gas strikes the
impregnated tobacco materials and intimately commingles therewith.
Additionally, an intact cellular structure capable of absorbing and
holding impregnating liquids within the tobacco cells for
subsequent expansion appears to be a primary requirement. It would
be expected that this procedure cannot be utilized successfully
with finely divided tobacco plant parts which usually make up a
reconsitututed tobacco product for the reason that such finely
divided materials have little of the typical intact cellular
structure of tobacco. Without such cellular structure there is
nothing available for cellular expansion by absorption of an
organic liquid and later heating. An additional difficulty for
adapting that process to reconstituted material is the fact that
the impact of a hot gas stream on a comminuted reconstituted
tobacco containing volatile hydrocarbons could easily reduce such a
material back to its original constituents, namely, tobacco fines
and dust.
A patent to Halter et al., U.S. Pat. No. 3,528,434, describes a
process whereby a water-soluble thermogelling gum is added to an
aqueous tobacco slurry containing dissolved air. The gum acts as an
adhesive and binding agent. On heating the mixture, the
thermosetting gums are stated by the patentee to gel before the
dissolved air escapes to form air channels in the tobacco
sheet.
It must be assumed that this process seeks to produce a porous
tobacco sheet which differs from a foamed sheet producd by the
escape of foaming agents. Additionally, the use and eventual
retention of the thermogelling gums could easily contribute a
foreign note to the smoke since it is a component part of the final
product. Such gums being foreign elements and even if innocuous
would be expected to reduce tobacco flavor and impact when such a
product is smoked.
An object of the present invention is to provide a simplified and
inexpensive process for increasing the filling capacity of
reconstituted tobacco.
Another object of the present invention is to provide a process for
producing an expanded, spongy reconstituted tobacco product free of
non-tobacco substances producing undesired foreign notes in the
tobacco.
These and other objects and advantages will become apparent from
the description of the invention which follows.
SUMMARY OF THE INVENTION
The present invention relates to a spongy expanded reconstituted
tobacco product and a process for producing it, in which an aqueous
slurry of finely divided tobacco plant particles and a pectin
binding agent derived from tobacco is commingled with a relatively
low boiling volatilizable aliphatic hydrocarbon or mixture of
hydrocarbons. A small amount of special emulsifier may be added to
aid the dispersion. The mixture is then cast or extruded into web
or sheet form and then heated to remove both water and
hydrocarbons. The volatilization causes expansion of the spaces
between the tobacco particles. The final dried product is a spongy
tobacco material of high porosity, with substantial filling power,
and may be prepared so that it contains no more than small amounts
if any of non-tobacco elements, and free of residual foaming
agents, foam stabilizers, non-tobacco celluloses, gums or
proteins.
DESCRIPTION OF THE INVENTION
In accordance with the invention, the starting material is what is
usually waste material in the form of tobacco shreds, scraps, dust
and fines. The tobacco parts are slurried in an aqueous medium and
then preferably refined to small particle sizes usually obtained in
preparing a reconstituted tobacco. To this slurry is added a
tobacco-derived binding agent either from extraneous sources or one
preferably developed in situ by any of the procedures as taught by
such patents as Hind et al., U.S. Pat. No. 3,353,541 or in U.S.
Pat. No. 3,420,421. These patents teach the treatment of tobacco
parts with specific reactants under conditions capable of releasing
tobacco pectins. The latter act as excellent binding agents when
combined with tobacco fines in the process of forming a
reconstituted tobacco sheet or product. The following explanation
will illustrate the procedure for obtaining a suitable binding
agent derived from tobacco which will bond and hold tobacco fines
into a coherent mass that can then be expanded by the process of
this invention to provide a spongy, porous web or sheet of
reconstituted tobacco.
It is known that pectin substances are present in tobacco in the
form of protopectins, comprising calcium and magnesium salts of
partially esterified and acetylated polymers of galacturonic acid.
On treatment of the tobacco with a non-toxic reagent such as an
alkali metal carbonate, or with selected chelating agents such as
ethylenediamine tetraacetic acid, or with an acid such as
hydrochloric or phosphoric acid, the protopectin cross-linking
chains are broken and tobacco pectins are released.
A particularly advantageous reactant, combining the
chain-destroying action with chelating action for removal of the
alkaline earth metal cross links is diammonium hydrogen phosphate
(DAP). This particular pectin releasing agent is preferred since it
is not only effective in relatively small amounts but more
importantly does not effect the final product in any noticeable way
if the products of the pectin releasing action are retained
therein. When using other tobacco pectin releasing agents, the
liberated pectins may be separated from the treating solution and
then added to tobacco fines as a binding agent. Alternatively,
where the precipitating agent or reaction products do not affect
the final product to an appreciable extent, the tobacco pectins may
be released and deposited with the treated tobacco in situ without
separation from the treating solution. Such procedures are fully
described in both of the Hind et al patents identified previously
and in both patents the advantages of using a tobacco binding agent
composed of tobacco pectins is fully described.
Where an in situ reaction is carried out leading to the release of
tobacco binding agents, the operation is generally carried out at
relatively high temperatures. Consequently, before the addition of
low boiling hydrocarbons, the next and important step is to cool
the slurry of tobacco dust and binding agent to lower temperatures,
namely, below 100.degree.C. and preferably in the range of about
20.degree. to 80.degree.C., and more preferably in the range of
about 25.degree. to 40.degree.C. It should be understood that
whether the tobacco binding agent is prepared in situ, or whether
it is obtained from other sources and added to the tobacco dust
slurry, the temperature of the mixture should for good results, be
adjusted to encompass the range indicated above. Experimental
evidence has shown that a substantially thicker and more expanded
product could be made if the temperature of the slurry is held to
about normal room temperature levels throughout the further
additions and up to the time the tobacco slurry reaches the heating
and drying stage.
To the cooled aqueous slurry of tobacco and binding agent is then
added a low boiling, hydrophobic, aliphatic hydrocarbon of about
five to eight carbon atoms as a foaming agent. Any straight or
branched-chain hydrocarbon may be selected that falls within the
boiling range of about 35.degree. to 125.degree.C. Such an agent
may easily be removed by evaporation under relatively non-drastic
heating or drying conditions as such or in the form of a water
azeotrope. Preferred hydrocarbons are the pentanes, hexanes, and
heptanes or mixtures thereof, such as petroleum ether or the like.
The amount of hydrocarbon added to the aqueous tobacco slurry
should be kept to a minimum and used only in sufficient amount to
expand the tobacco without leaving a residue. This may range from
about 0.007 to no more than about 7.0 parts per 100 parts by weight
of the tobacco fines. Less than this amount results in poor
expansion and more than this amount tends to result in some
residual material remaining in the tobacco sheet or will result in
a weak and lacy tobacco sheet or such fragility as to reduce the
sheet to tobacco fines. A preferred range of aliphatic hydrocarbon
is from about 0.07 to about 1.5 parts of hydrocarbon per 100 parts
by weight of the tobacco.
The hydrocarbons that are added to the aqueous slurry are
intimately dispersed throughout the medium preferably by a high
speed mixer or blendor device. If relatively large particles are
present the slurry may be further beaten or refined. To aid in
obtaining a good dispersion or emulsion of the hydrophobic agent
with the aqueous medium, a small amount of a special emulsifier may
be added to the slurry of tobacco fines and hydrocarbon in an
amount of about 5 percent by weight or less, and preferably from
about 0.5 to 2.5 percent by weight based on the tobacco content in
the slurry.
In the use of an emulsifying agent in the exercise of this
invention, the emulsifying agent must be selected with care, not
only for its effectiveness in dispersing the hydrophobic agent in
the aqueous medium and effecting an emulsified mixture, but
particularly with respect to its residual contribution to the final
reconstituted tobacco product. Since the emulsifier is generally
too high-boiling to volatilize out when the hydrocarbon component
is removed by low temperature heating, it remains as a residual
component that could, if not carefully selected as to type and
amount, affect the smoking characteristics of the final foamed
product by a possibly unpleasant aroma or by effecting an
unpleasant "mouth coating." This expression is used in the tobacco
art to refer to an orally unpleasant sensation that something is
present on the inside of the smoker's mouth.
It is therefore critical with respect to the present invention,
that when an emulsifier is used it should be selected to produce a
well emulsified mixture so efficiently that very small amounts are
necessary. Preferably the emulsifier will also impart either a
desirable and delicate flavor to the tobacco, or to improve and
enhance the flavor and aroma of the tobacco.
Thus, in accordance with the emulsification aspect of the
invention, one emulsifier has been found that also imparts an
intriguing flavor to tobacco smoke. Such an emulsifier is licorice
or salts of this material, such as ammonium glycerrhizinate.
Another type of emulsifier that also adds to the tobacco flavor is
a mixture of resins obtained from tobacco itself.
Licorice or glycyrrhizin salts, such as ammoniated glycyrrhizin are
commercially available. Tobacco resins are obtained by known
procedures, usually by extraction of tobacco with organic solvents
such as hexane. These resins contain fatty acids, esters and salts
that not only act as effective emulsifiers but may be added in an
amount to result in enhancement of the tobacco flavor and
aroma.
These flavoring emulsifying agents are effective emulsifiers in an
amount of about 1 to 5 percent by weight of the tobacco slurry and
generally in an amount of less than 3 percent by weight. Actually,
it has been found that these agents produce effective results when
used in an amount of as little as about 0.25 to 1 percent by weight
based on the tobacco.
In addition to the above flavor emulsifiers there are certain
innocuous or non-flavor emulsifiers that are fairly efficient
emulsifying agents and effective in such small amounts that their
impact in the final product is imperceptible. Thus, it has been
found that stearic acid or lauric acid or lauryl ether sulfate, or
the alkali or alkaline earth metal salts thereof fall within this
group. Emulsifiers of this type are effective when used in an
amount below 1 percent by weight of the tobacco, an effective range
for satisfactory emulsification being from about 0.0002 g to about
0.2 g per 100 g of tobacco.
While the various emulsifiers mentioned above are preferably used
singly if at all, they may also be used in admixture as long as the
amounts do not exceed the upper limits given for the flavor type or
the non-flavor type of emulsifiers.
The tobacco slurry, containing the binding agent and the
low-boiling hydrocarbons is subjected to a high speed mixing and
refining operation to obtain a homogeneous dispersion of the
ingredients in the aqueous medium. A Cowles dissolver with a high
shear impeller or a Waring blendor may be used for the mixing step.
Little if any foaming or entrapment of air takes place during the
high speed dispersion since only very small quantities of
dispersing agents are needed or used in the process. Following the
high speed mixing step, the slurry is brought to below
100.degree.C. or preferably room temperature if above this point.
One then adds the volatilizable aliphatic hydrocarbon agent or
agents, and preferably also the emulsifying agent. The entire
mixture is again thoroughly dispersed or emulsified.
Following the effective dispersion of the hydrophobic agent
throughout the slurry mixture, the dispersion mixture is then
forwarded to a heating and foaming zone for forming a foamed,
spongy sheet or web of reconstituted tobacco. Any conventional
heating means for drying a tobacco slurry to form a reconstituted
sheet may be used. One may use radiant energy heating such as that
provided by infrared heating means or by using heated surfaces
where the tobacco-hydrocarbon dispersion is cast or extruded onto
metal plates or a moving stainless steel belt generally heated from
the botton with steam or hot gases.
The heating of the tobacco sheet containing the dispersed
hydrocarbons causes the hydrocarbons or the hydrocarbon-water
azeotrope to volatilize into gaseous or vapor form and in escaping,
forms cavities between the interstices of the tobacco particles
producing a substantially expanded product. The heating step is
carried out at a temperature in the range of about 150.degree. -
240.degree.F. preferably from 180.degree. - 220.degree.F. When a
moving belt is used, the speed of travel through the heating area
may be 1 to 18 ft/min., and preferably 2-8 ft/minute. The dried
product in the form of an expanded web or sheet may be removed
using a doctor knife.
In the heating and drying operation, the temperature of drying
causes the tobacco fines in conjunction with the tobacco pectin
binding agent to cohere. Additionally, the low boiling hydrocarbons
and water foam and volatilize off, forming cavities and expanded
areas when viewed in cross-section, thereby resulting in a porous,
spongy, product with a uniform color similar to natural tobacco
leaf. Reconstituted tobacco sheet made in the usual manner is
generally darker on top than on the belt side with the latter being
mottled. A surprising characteristic of the product produced by the
present method is its porosity and sponginess. In point of fact, it
is so spongy and porous that a drop of water placed on its surface
is absorbed as though by blotting paper.
Physical tests of the products produced by the present invention
show a substantially lower density and greater thickness than that
obtained in reconstituted tobacco sheet made by the usual methods.
In one such test, density measurements may be carried out by
weighing oven-dry material, then conditioning at 25.degree.C. to 60
percent relative humidity for thickness measurement to avoid
breakage. Density may be designated in g/sqft/10 mil thickness,
although one may select any thickness from 1 to 100 mils provided
all density measurements are calculated to the same thickness. In
carrying out the present invention, the products produced
demonstrated materially reduced densities over controls of unfoamed
reconstituted tobacco tested under similar conditions.
When the products are compared to unfoamed reconstituted tobacco
controls on a thickness basis, the products of the invention
measured substantially thicker as well as more spongy than the
controls. Moreover, in testing the products for wet strengths, the
products of the invention possessed a wet strenth well above
1.0/g/in/g/sq ft which permits subsequent processing of the sheet
on standard equipment without difficulties.
The reconstituted foamed product, when prepared without the use of
an emulsifier or when a fatty acid type of emulsifier was used,
when cut or shredded to make cigarets, required less tobacco and
provided a smoke that was indistinguishable from control cigarets
prepared with ordinary reconstituted tobacco. There were no notes
foreign to tobacco that could be detected in the prepared cigaret.
Moreover, the product blended well with tobacco leaf filler. When
the reconstituted foamed product was prepared using a flavoring
type of emulsifier, the flavor of the tobacco was not only
desirably enhanced but the product also possessed a substantially
increased filling capacity and much lower density than ordinary
reconstituted tobacco.
The following examples are illustrative of the invention. All parts
as given below should be understood to be parts by weight unless
otherwise designated.
EXAMPLE 1
Three hundred grams of tobacco slurry was prepared by mixing in a
blendor 10 parts of tobacco fines, 0.8 parts diammonium hydrogen
phosphate (DAP), 1.6 parts of aqueous ammonia (30 percent NH.sub.3)
and 87.5 parts of water. The slurry was heated for one hour in a
steam bath, refined for 10 minutes, and cooled to room temperature.
Additional ammonia was added to maintain pH 9.0 during the heating
period. After the cooling, the slurry was mixed for five minutes
while 0.6 g of licorice powder and 0.15 ml heptane were added.
After the mixing, the slurry was cast on stainless steel plates
using a casting knife with a 50-mils setting, dried over a steam
bath, and doctored off the plates. Sheet weight in grams per square
foot was determined on the bone-dry material, and calculated for 10
mils thickness (a density index). Thickness of the sheet material
that was equilibrated at 60 percent RH and 25.degree.C. was
measured with a model 549 micrometer, (Testing Machines, Inc.
Amityville, L.I., N.Y.). The sheet was 11.95 mils thick and weighed
11.68 g/sq ft/10 mils. The sheet was spongy and porous. It had a
similar color both on the plate and top sides, and resembled a dark
natural tobacco leaf.
A control sheet was prepared as above but without the addition of
licorice and heptane. This sheet was 8.66 mils thick and weighed
16.21 g/sq ft/10 mils. The top side of this sheet was dark, while
the plate side was light in color and somewhat mottled.
EXAMPLES 2-7
In each of these six examples, 300 g of tobacco slurry was prepared
as in Example 1, except the licorice amounts were varied from none
to 1.5 grams and the heptane level was 0.15 ml in all cases. The
casting and drying operation was carried out without delay.
The results are shown in Table 1. The color of the sheets in this
series was similar for both sides and resembled natural dark
tobacco leaf. The sheets were thicker and weighed less than the
control.
TABLE 1
Licorice Sheet Example Added Thickness Weight No. g mils g/sq ft/10
mils Control* 8.66 16.21 2 -- 10.73 13.29 3 1.5 12.23 11.19 4 1.2
12.10 12.93 5 0.9 12.50 11.59 6 0.15 11.64 12.56 7 0.075 11.51
12.36 *Control without heptane of licorice
It will be noted from these examples that an improved product, as
compared to the control was produced even when an emulsifier was
not used since the dispersion was not permitted to separate or
break and lose heptane unduly. It will be noted, however, that when
using the licorice emulsifier a lower density and thicker product
was obtained. It will be further noted that increasing amounts of
emulsifier generally caused a decreasing density and a thicker
product.
EXAMPLE 8
The tobacco slurry was prepared as in Example 1 except 1.20 g.
ammoniated glycyrrihizin and 0.60 ml heptane were added to 800 g
slurry, and the slurry was cast at 35 mils instead of 50 mils. A
control was also prepared.
Sheet Thickness Sheet Weight mils g/sq ft/10 mils Control 7.0 13.0
Treated 8.5 11.3
EXAMPLE 9
The tobacco slurry was prepared as in Example 1, and maintained at
80.degree.C. One hundred grams of the slurry was mixed for five
minutes after adding 3.0 g of tobacco resins (hexane solubles).
After the mixing, additional 200 g of slurry was added, and
blended. When the mixture was cooled to 50.degree.C., 0.60 ml
heptane was added with additional blending for five minutes, then
cast on stainless steel plates using a casting knife with a 50 mils
setting. The process was completed to yield the treated sheets.
Control sheets were also prepared containing the added tobacco
resins, but no heptane.
Sheet Thickness Sheet Weight mils g/sq ft/10 mils Control 8.4 18.2
Treated 14.4 11.1
The treated sheets were lighter and more uniform in color than the
controls.
EXAMPLE 10
Three hundred grams of tobacco slurry was prepared as in Example 1
and cooled to room temperature. To the slurry were added 0.15 g
stearic acid and 0.30 ml heptane, then mixed for five minutes. It
was cast on stainless steel plates using a casting knife set at 50
mils and processed to yield the treated product. A control product
was also prepared without stearic acid or heptane.
Sheet Thickness Sheet Weight mils g/sq ft/10 mils Control 8.63
15.85 Treated 11.87 11.25
EXAMPLE 11
A tobacco slurry was prepared using a generally similar procedure
to that described in U.S. Pat. No. 3,353,541 or U.S. Pat. No.
3,420,241 for obtaining tobacco pectins. Thus, to 80 parts of water
at 195.degree.C., 16 part of tobacco fines, 1.3 parts of DAP, and
2.6 parts of aqeous NH.sub.3 (30% NH.sub.3) were added. The mixture
was stirred for one hour and subsequently refined in a disk type
refiner. Additionaly NH.sub.3 was added to maintain a pH of 9.0.
The slurry was cooled to room temperature, three hundred grams of
the slurry was transferred into 200 ml water in which was dispersed
0.1 g calcium searate and 5 ml heptane, thereby providing about 0.2
g of calcium stearate and about 7 g of heptane per 100 g of tobacco
dust. The mixture was stirred until it appeared homogeneous,
usually about 5-10 minutes, cast on stainless steel plates using a
casting knife with a 50 mils setting, dried over a steam bath, and
doctored off the plates. The sheet was 14.0 mils thick and weighed
9.0 g/sq ft/10 mils. The color was similar on both sides, and the
sheet had good physical characteristics as to wet tensile strength,
texture and porosity.
A control without calcium stearate or heptane was prepared as
above. This sheet was 9.0 mils thick and weighed 16.3 g/sq ft/10
mils. It was a dense sheet with the top side much darker than the
steel plate side.
The reconstituted tobacco sheets were shredded and prepared into
hand made cigarets. When smoked, the smoke of the experimental and
control cigarets appeared the same. There was no evidence of any
mouth coating from either cigaret.
EXAMPLES 12-14
In Example 12, 50 g of the above slurry as prepared in Example 11
with calcium stearate and heptane was dispersed in a blendor
containing 200 ml of water. To this was added 300 g of the original
concentrated tobacco slurry without additional calcium stearate or
heptane, and mixed until homogeneous, usually 5-10 minutes. This
mixture contained approximately 0.01 g calcium stearate and 0.5 ml
heptane, thereby providing approximately 0.02 g of calcium stearate
per 100 g. of tobacco dust. The tobacco sheets were prepared as in
Example 11. Results are shown in Table 2.
In Example 13, 50 g of surry as prepared in Example 12 was
dispersed in a blendor containing 200 ml water. To this was added
300 g of the original concentrated tobacco slurry and treated as in
Example 12. The final mixture contained approximately 0.001 g
calcium stearate (0.002 g/100 g tobacco dust) and 0.05 ml heptane.
Results are shown in Table 2.
In Example 14, 50 g of slurry as prepared in Example 13 was
dispersed in a blendor containing 200 ml water. To this 300 g of
the original concentrated tobacco slurry was added and processed as
in Example 12. The final mixture contained approximately 0.001 g
calcium stearate (0.0002 g/100 g tobacco) and 0.005 ml heptane
(0.0068 g/100 g tobacco). Results are shown in Table 2.
TABLE 2
Example Calcium Thick- No. Sterate Heptane ness Weight g ml mils
g/sq ft/10 mils Control* -- -- 9.0 16.3 12 0.01 0.5 11.0 11.3 13
0.001 0.05 10.0 11.2 14 0.0001 0.005 9.5 15.5 *No calcium sterate
or heptane
EXAMPLE 15
Twenty-one hundred grams of tobacco slurry was prepared as in
Example 1 and allowed to cool to room temperature. Three hundred
grams of the prepared slurry was mixed in a blendor for five
minutes, then cast on stainless steel plates using a casting knife
set at 50 mils. The process was carried to completion to yield the
control tobacco sheet. To another 300 g portion of the slurry was
added 0.15 g sodium lauryl ether sulfate and 1.5 ml heptane and
mixed for five minutes. This tobacco slurry was cast and processed
to yield the experimental tobacco sheet.
Wet Tensile Thickness Weight Coefficient mils g/sq ft/10 mils
g/in/g/sq ft Control 7.4 19.0 7.8 Experimental 12.8 11.6 1.9
The experimental sheet was light in color and similar on both
sides, whereas the control sheet was dark on the top and mottled on
the plate side. The wet tensile coefficient is sufficient for
processing the sheet into cigarettes using machinery that is
current in the cigaret industry today.
EXAMPLES 16-20
The procedure in Example 15 was repeated using 300 g portions of
the prepared slurry to each of which 0.15 g sodium lauryl ether
sulfate and varied levels of hydrocarbon foaming agent were added.
The heptane levels ranged from 0.30 ml to 0.003 ml. The mixtures
were blended, cast and dried to yield the experimental tobacco
sheets.
TABLE 3
Heptane Thick- Wet Tensile Example Added ness Weight Coefficient
No. ml mils g/sq ft/10mils g/in/g/sq ft 16 0.30 13.5 11.0 5.3 17
0.15 12.5 11.1 5.5 18 0.03 10.3 13.8 6.2 19 0.015 8.8 15.3 5.8 20
0.003 8.3 16.0 7.3
EXAMPLE 21
The tobacco slurry was prepared as in Example 1 and cooled to room
temperature. To 300 g of the slurry was added 0.30 g sodium lauryl
ether sulfate and 0.15 ml petroleum ether (density 0.64). After
mixing in a blendor for 10 minutes it was cast at 50 mils on
stainless steel plates, dried over a steam bath and doctored off
the plates. Control sheets without the lauryl ether sulfate or
petroleum ether were also prepared.
Sheet Thickness Sheet Weight mils g/sq ft/10 mils Control 10.2 14.6
Treated 16.2 10.2
EXAMPLE 22
Eight hundred grams of tobacco slurry was prepared as in Example 1.
After cooling the slurry, 0.80 g sodium lauryl ether sulfate and
0.30 heptane were added and mixed for 5 minutes in a blendor. After
mixing, the slurry was passed at 6000 psi through a Manton-Gaulin
homogenizer Model 15A8BASMD (Manton-Gaulin Mfg. Co., Inc. Averett,
Mass.) and immediately cast on stainless steel plates using a
casting knife with a 35-mils setting. These sheets were then dried
over a steam bath and doctored off the plates. A control was also
prepared in the same manner as above, but no lauryl ether sulfate
or heptane were added to the slurry.
Thickness Weight mils g/sq ft/10 mils Control 5.26 19.65
Experimental 11.51 9.38
The experimental product was uniform and light in color whereas the
control was dark on the top and mottled on the plate side.
The reconstituted fllms were shredded and hand made cigarets
prepared. The smoke flavor of the experimental cigaret was
indistinguishable from that of the control. The additives in the
experimental had no apparent effect on smoke flavor characteristics
nor was mouth coating noted.
EXAMPLES 23-26
Temperature Variation
Four hundred grams of tobacco slurry was prepared by mixing in a
blendor 10 parts tobacco fines, 0.8 parts DAP, 0.1 parts
triethylene glycol, three parts of aqueous ammonia (30 percent
NH.sub.3) and 86.1 parts water. The slurry was heated for one hour
on a steam bath, refined for ten minutes (pH maintained at 9.5),
and cooled to 80.degree.C. To this mixture 0.2 g sodium lauryl
ether sulfate and 0.2 ml heptane were added and mixed for five
minutes. The slurry was then cast on stainless steel plates using a
casting knife with a 35-mils setting, dried over a steam bath and
doctored off the plates. A control was prepared as above but
without the lauryl ether sulfate and heptane. Sheet thickness and
weight were determined and the percentage increase in thickness and
decrease in weight were calculated. Results are shown in Table
4.
The above procedure was repeated except the slurries were cooled to
60.degree.C., 40.degree.C., and 20.degree.C. at the time of
addition of lauryl ether sulfate and heptane just prior to casting.
Controls were also prepared for each corresponding temperature.
Experimental films were uniform in color with both sides similar.
The control films were dark on the top side and mottled on the
plate side.
TABLE 4
Thickness Weight Weight Increase Decrease Casting g/sq Above Below
Example Temp. ness ft/10 Control Control Number .degree.C. mils
mils % % 23 80 8.10 11.28 55.8 29.6 Control* 80 5.20 16.02 24 60
9.77 8.90 101.0 49.2 Control* 60 4.86 17.53 25 40 12.83 6.66 168.4
61.4 Control* 40 4.78 17.24 26 20 12.63 6.64 166.5 60.9 Control* 20
4.74 17.00 *No added lauryl ether sulfate or heptane.
The results of this group of examples (23-26) indicate that
temperatures of the slurry after blending with binding agent and
before the addition of hydrocarbons for foaming should be well
below 1002 C. and temperature adjustment to a lower level should be
carried out and maintained until the combined slurry mixture passes
to the heating and drying stage.
* * * * *